Gas-Liquid Chromatographic Determination of Nifursol in Frozen Turkey Tissues to Ten Parts Per Billion

1975 ◽  
Vol 58 (4) ◽  
pp. 694-699
Author(s):  
Larry J Frahm ◽  
Glenn M George ◽  
J Patrick Mcdonnell
Keyword(s):  
Ethyl Acetate ◽  
Chromatographic Determination ◽  
Peak Height ◽  
Gas Liquid Chromatography ◽  
Method Performance ◽  
Florisil Column ◽  
Column Eluate ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract Nifursol (3,5-dinitrosalicylic acid (5-nitrofurfurylidene) hydrazide) is extracted into ethyl acetate from 10 g tissue in the presence of sodium sulfate. Tissue interferences are removed from the tissue extract by washing with petroleum ether after the extract has been transferred into an aqueous solution by evaporation of ethyl acetate. The drug is hydrolyzed under acid conditions to form 5-nitro-2-furaldehyde (5NF). After partition of 5NF from the aqueous phase into benzene the extract is further cleaned up on a Florisil column. The 5NF is eluted from the Florisil column with benzeneethyl acetate. Electron capture gas-liquid chromatography of a 10 μl injection of the concentrated column eluate is the determinative step. Quantitation is accomplished by comparison of the peak height of the sample to the peak height of the standard which is carried through the method simultaneously. Studies of method performance on turkey muscle, liver, kidney, and skin tissues fortified to contain 10 ppb nifursol show a recovery range of 87.4–95.0% and a coefficient of variation range of 5.7–11.2%.

Gas-Liquid Chromatographic Determination of Kepone in Field-Collected Avian Tissues and Eggs

1978 ◽  
Vol 61 (1) ◽  
pp. 08-14 ◽  
Author(s):  
Charles J Stafford ◽  
William L Reichel ◽  
Douglas M Swineford ◽  
Richard M Prouty ◽  
Martha L Gay
Keyword(s):  
Mass Spectrometry ◽  
Chromatographic Determination ◽  
Bald Eagle ◽  
Gas Liquid Chromatography ◽  
Tissue Samples ◽  
Florisil Column ◽  
Average Recovery ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A procedure is described for determining Kepone (decachlorooctahydro-l,3,4-metheno-2H-cyclobuta [cd]pentalene-2-one) residues in avian egg, liver, and tissue. Samples were extracted with benzene-isopropanol, and the extract was cleaned up with fuming H2SO4-concentrated H2SO4. Kepone was separated from organochlorine pesticides and polychlorinated biphenyls on a Florisil column and analyzed by electron capture gas-liquid chromatography GLC). The average recovery from spiked tissues was 86%. The analyses performed on 14 bald eagle carcasses and livers, 3 bald eagle eggs, and 14 osprey eggs show measurable levels which indicate that Kepone accumulates in the tissues of fish-eating birds. Residues were confirmed by GLC-mass spectrometry.

Gas-Liquid Chromatographic Determination of Permethrin in Bovine Tissues

1979 ◽  
Vol 62 (6) ◽  
pp. 1309-1311
Author(s):  
Delbert D Oehler
Keyword(s):  
Liquid Chromatography ◽  
Electron Capture ◽  
Chromatographic Determination ◽  
Chromatographic Column ◽  
Gas Liquid Chromatography ◽  
Florisil Column ◽  
Bonded Phase ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A method is presented for the determination of permethrin (m-phenoxybenzyl cis,trans-(±)-3-(2,2-dichlorovinyl) - 2,2 - dimethylcyclopropanecarboxylate) in bovine tissues. Fat and muscle samples were cleaned up first by liquid-liquid partition on a bonded phase chromatographic column. Final cleanup of fat and muscle was performed on a short Florisil column. Liver, kidney, spleen, and heart tissues only required cleanup on a Florisil column before quantitation of permethrin by electron capture gas-liquid chromatography.

Gas-Liquid Chromatographic Determination of Thiabendazole and Methyl 2-Benzimidazole Carbamate in Fruits and Crops

1979 ◽  
Vol 62 (4) ◽  
pp. 769-773 ◽  
Author(s):  
Gwan H Tjan ◽  
John T A Jansen
Keyword(s):  
Ethyl Acetate ◽  
Chromatographic Determination ◽  
Gas Liquid Chromatography ◽  
Liquid Chromatography Mass Spectrometry ◽  
Liquid Liquid Extraction ◽  
Alumina Column Chromatography ◽  
Pentafluorobenzyl Bromide ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A method is described for the electron capture gas-liquid chromatographic determination of thiabendazole and methyl 2-benzimidazole carbamate (MBC) after derivatization with pentafluorobenzyl bromide (PFB-Br). The samples are extracted with ethyl acetate, and the residual thiabendazole, benomyl, and MBC are isolated by liquid-liquid extraction into dilute HC1. After neutralization and re-extraction with ethyl acetate, thiabendazole and MBC are reacted with PFB-Br to form the PFB derivatives. Alumina column chromatography was used to clean up extracts, and the derivatives could be detected as low as 5–10 pg. Recoveries were 95-98% from fruits fortified with 0.3-2.0 ppm thiabendazole; recoveries were 91–97% when 0.05–1.0 ppm benomyl/MBC were added to fruits/crops. The PFB derivatives were identified by gas-liquid chromatography-mass spectrometry.

Gas-Liquid Chromatographic Determination of Pydrin, a Synthetic Pyrethroid, in Cabbage and Lettuce

1978 ◽  
Vol 61 (4) ◽  
pp. 869-871
Author(s):  
Young W Lee ◽  
Neil D Westcott ◽  
Randy A Reichle
Keyword(s):  
Liquid Chromatography ◽  
Petroleum Ether ◽  
Electron Capture ◽  
Chromatographic Determination ◽  
Synthetic Pyrethroid ◽  
Gas Liquid Chromatography ◽  
Florisil Column ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract Pydrin, a-cyano-3-phenoxybenzyI 2-(4-chlorophenyl)-3-methylbutyrate, a synthetic pyrethroid ester, is extracted from vegetables with acetonitrile, partitioned into petroleum ether before cleanup on a Florisil column, and analyzed by electron capture gas-liquid chromatography. Recoveries of 88-102% at 0.01 ppm, 99-102% at 0.1 ppm, and 98—104% at 1.0 ppm were obtained from fortified cabbage and lettuce samples. The method appears applicable to detection of the residues of Pydrin in the foliage of many types of crops.

Collaborative Study of the Quantitative Gas-Liquid Chromatographic Determination of Fusel Oil and Other Components in Whisky

1972 ◽  
Vol 55 (3) ◽  
pp. 549-556
Author(s):  
J H Kahn ◽  
E T Blessinger
Keyword(s):  
Ethyl Acetate ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
Official Method ◽  
Fusel Oil ◽  
Fusel Alcohols ◽  
Aoac Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract Fifteen chemists participated in a collaborative study for the quantitative pas-liquid chromatographic determination of the individual fusel alcohols and ethyl acetate in whisky. Two levels of congeners represented by 4 coded samples of whisky were analyzed by using t h e proposed method, employing a glycerol-1,2,6-hexanetriol column, and the official AOAC method, 9.063-9.065. Since isobutyl and the atnyl alcohols comprise by far the greatest part of fusel oil, their determination is of major importance to the total fusel oil content . Statistical analyses show that the proposed method is superior to the AOAC method for the determination of these alcohols, whereas the official method is superior for the determination of ethyl acetate and n-propyl alcohol. In general, collaborators employing modern instrumentation preferred the proposed method over the AOAC method. The former method also separates and permits the quantitative measurement of active amyl and isoamyl alcohols. The proposed method has been adopted as official first action as an alternative to 9.063–9.065 for the determination of higher alcohols and ethyl acetate in whisky.

Gas-Liquid Chromatographic Determination of Sodium Fluoroacetate (Compound 1080)

1980 ◽  
Vol 63 (1) ◽  
pp. 49-55
Author(s):  
Iwao Okuno ◽  
Dennis L Meeker
Keyword(s):  
Liquid Chromatography ◽  
Tissue Sample ◽  
Chromatographic Determination ◽  
Gas Liquid Chromatography ◽  
Tissue Samples ◽  
Fluoroacetic Acid ◽  
Pentafluorobenzyl Bromide ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract An analytical method is described for the determination of Compound 1080 (sodium fluoroacetate) residues in 1–10 g tissue. Sample extracts of tissues are cleaned up with silica gel, and Compound 1080 (as fluoroacetic acid) is separated by a micro-distillation procedure. The fluoroacetic acid in the distillate is derivatized with pentafluorobenzyl bromide to form pentafluorobenzyl fluoroacetate which is measured by electron capture gas-liquid chromatography. Recoveries of sodium fluoroacetate from fortified tissue samples averaged about 25%. Despite the limited recoveries, results were quite reproducible, and levels as low at 2 ppm were determined in fortified 1 g samples, and 0.2 ppm in 10 g samples. The method is relatively simple and has been used routinely in our laboratory for the analysis of various types of samples such as grain, and tissues from birds, rodents, and larger animals.

Gas-Liquid Chromatographic Determination of Maleic Hydrazide in Tobacco and Tobacco Smoke

1979 ◽  
Vol 62 (1) ◽  
pp. 171-175 ◽  
Author(s):  
Alfred F Haeberer ◽  
Orestes T Chortyk
Keyword(s):  
Liquid Chromatography ◽  
Tobacco Smoke ◽  
Plant Growth Regulator ◽  
Maleic Hydrazide ◽  
Chromatographic Determination ◽  
Gas Liquid Chromatography ◽  
Trimethylsilyl Derivative ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A method is presented for the determination of the plant growth regulator maleic hydrazide (MH; l,2-dihydro-3,6-pyridazinedione) in tobacco and tobacco smoke. Residues are converted to the bis(trimethylsilyl) derivative before analysis by gas-liquid chromatography. The method has been applied to cigarettes and condensed smoke and has been used to determine the per cent transfer of MH into cigarette smoke. Free MH residues could be determined directly on the tobacco samples, whereas total MH values were obtainable only after acid hydrolysis. In spite of large MH residues in tobacco, only 0.2% of the MH was transferred into smoke.

Liquid Chromatographic Determination of Quinine, Hydroquinine, Saccharin, and Sodium Benzoate in Quinine Beverages

1985 ◽  
Vol 68 (4) ◽  
pp. 782-784
Author(s):  
Leonard P Valenti
Keyword(s):  
Sodium Benzoate ◽  
Direct Injection ◽  
Chromatographic Determination ◽  
Peak Height ◽  
Relative Standard ◽  
Sodium Saccharin ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
The Relationship

Abstract A liquid chromatographic (LC) method is described for the determination of quinine, hydroquinine, sodium saccharin, and sodium benzoate in soft drinks. The method involves simple sample preparation, direct injection onto an octadecylsilane column, and elution with a methanol-acetonitrile-water-acetic acid (20 + 10 + 70 + 1) mobile phase. Eluted constituents are measured spectrophotometrically at 254 nm. The relationship between peak height and concentration was linear between 20 and 120 μg/mL for quinine. A relative standard deviation of 0.82% was obtained for commercial samples spiked with quinine, and the average recovery was 100.3%. The proposed procedure is accurate and rapid and can also detect hydroquinine (a natural contaminant of quinine), sodium saccharin, and sodium benzoate. Linear responses ranged from 0.45 to 20 (xg/mL for hydroquinine, from 54.8 to 219 μg/mL for sodium saccharin, and from 10.1 to 145.1 (ig/mL for sodium benzoate. The reproducibility of the LC method was evaluated with standard solutions of hydroquinine, sodium saccharin, and sodium benzoate, which produced relative standard deviations of 0.42, 0.46, and 1.13%, respectively. The average recoveries for sodium saccharin and sodium benzoate from spiked samples were 99.4 and 100.2%, respectively.

scholarly journals Liquid Chromatographic Determination of α-Solasonine in Frozen Green Peas as an Indicator of the Presence of Nightshade Berries

2003 ◽  
Vol 86 (4) ◽  
pp. 759-763 ◽  
Author(s):  
Peter Cavlovic ◽  
Mohan Mankotia ◽  
Peter Pantazopoulos ◽  
Peter M Scott
Keyword(s):  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Solanum Nigrum ◽  
Expanded Uncertainty ◽  
Method Performance ◽  
Limit Of Quantitation ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Green Peas

Abstract Nightshade berries containing glycoalkaloids can be a contaminant in green peas. Methodology was developed to detect this contamination. The glycoalkaloid α-solasonine was extracted from frozen green peas with 1% (v/v) acetic acid, cleaned up on a C18 cartridge, and determined by liquid chromatography with UV detection at 200 nm. Method performance characteristics for the determination of α-solasonine include linearity from 140 to 1500 ng injected (r = 0.9996–0.9999); recovery ranging from 68 to 79%; limit of quantitation (LOQ) = 4.5 ppm (280 ng standard), and limit of detection = 0.64 ppm (40 ng standard). At the LOQ, the expanded uncertainty at 95% confidence was 0.38 × the reported value. The method was applied to the detection of α-solasonine in frozen green peas in a 2-year study of 60 samples of frozen green peas from Ontario, Canada. None of the samples contained α-solasonine. No unripe berries of Solanum nigrum were detected visually in the samples.

Rapid Extraction and Gas-Liquid Chromatographic Determination of Benzoic and Sorbic Acids in Beverages

1983 ◽  
Vol 66 (1) ◽  
pp. 209-211
Author(s):  
Ricardo G Coelho ◽  
David L Nelson
Keyword(s):  
Chromatographic Determination ◽  
Gas Liquid Chromatography ◽  
Benzoic Acids ◽  
Ethereal Extract ◽  
Rapid Extraction ◽  
Liquid Chromatographic Determination ◽  
Carbonated Drinks ◽  
Temperature Programmed ◽  
Liquid Chromatographic

Abstract A rapid method for extraction and quantitative determination of sorbic and benzoic acids in carbonated drinks and fruit juices is described. Acidified sample aliquots are transferred onto an Extrelut column. Acid preservatives are then eluted from the column with a mixture of ethyl ether-petroleum ether. Content of preservatives in the concentrated ethereal extract is readily determined by temperature-programmed gas-liquid chromatography without the need to prepare derivatives.

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